Oil release for 100% synthetic fibers

ABSTRACT

Soil release properties of a 100 percent synthetic textile are improved by impregnating the same with a mixture of polyacrylic acid and an essentially linear water-insoluble swellable synthetic polymer which absorbs at least 550 percent of water. Soil release properties of a 100 percent synthetic textile can also be improved by subjecting the textile to an alkaline scour followed by treatment with the water insoluble swellable polymer.

United States Patent Hinton, Jr. et a1.

[451 Mar. 21, 1972 [54] SOIL RELEASE FOR 100% SYNTHETIC FIBERS [72]inventors: Everett H. Hinton, Jr.; Larry E. Avery,

both of Greensboro, NC.

Burlington Industries, Inc., Greensboro, NC.

[22] Filed: July 25, 1968 [21] Appl.No.: 747,473

[73] Assignee:

[52] U.S.Cl. ..1l7/47 A, 8/l15.6, 8/1l6.3, 117/76 T, 117/62, 117/1385,117/1388 A,

117/1394, 117/1395 R [51] Int. Cl. ..D06m 15/36 [58] Field ofSearch..l17/47, 138.5, 138.8 A, 139.5 R, 117/1394, 76 T, 62; 8/1 15.6, 116.3

[56] References Cited UNITED STATES PATENTS 7/1962 Lauchenauer ..1 17/473,152,920 10/1964 Caldwell ..l17/138.8

3,236,685 2/1966 ..117/138 8 3,265,529 10/1966 ...l17/138.8 X 3,322,5695/1967 ..l17/139.5 X 3,377,249 4/1968 ..1l7/139.5 X

Primary Examiner-William D. Martin Assistant Examiner-William R. TrcnorAttorney-Cushman, Darby & Cushman [5 7] ABSTRACT 13 Claims, No DrawingsOIL RELEASE FOR 100% SYNTHETIC FIBERS The present invention is concernedwith the treatment of a textile material which is made up entirely ofsynthetic fibers in order to improve the soil or grease releaseproperties thereof.

It is well known that oilor grease-borne stains in fabrics composed ofsynthetic fiber, e.g., polyester fibers, are difficult to remove bylaundering, due in at least some measure to the hydrophobic nature ofthe fibers. Oil-borne stains can usually be removed by dry cleaning butthis is expensive and undesirable, particularly since an importantadvantage of fabrics containing synthetic fibers is that they retaintheir shape through laundering and need little, if any, ironing.

With the advent of durable press garments, whether of the post-cured orpre-cured" type, there has been considerable research activity directedtowards improving the grease or soil release properties of cellulosicfabrics, which usually comprise blends of cellulosic and syntheticfibers, because the nature of the durable press finish (e.g., aminoplastresin and catalyst) applied to the fabric tends to make soil, especiallygrease-type stains, more difficult to remove or release in launderingthan would normally be the case without the finish. As a result of thisresearch, various soil release'agents have been developed for additionto durable press finishing compositions which greatly improve the soilrelease properties of cellulosic/polyester blend fabrics. However, ithas been found that these soil release agents do not produce equallyeffective soil release on fabrics whose fiber content is entirelysynthetic, e.g., 100 percent polyester fabric. In particular, the soilrelease ratings do not reach the desired value after laundering and/orthe finish suffers from a lack of durability and is rendered ineffectiveas the fabric undergoes repeated washing. The exact reasons for this arenot understood but the lack of durability of the soil release finish maybe due to the fact that 100 percent synthetic fabrics are not normallyprovided with resin/catalyst durable press type finishes and thesefinishes may somehow improve adhesion of the soil release agent to thecellulosic/synthetic blends on which they are generally employed.Additionally, synthetic fibers, especially polyester fibers, do not havethe highly reactive sites that characterize cellulose; the surfaces ofsynthetic fibers are of a somewhat lower energy than cellulosics and,therefore, less wettable; and the absorption of cellulosics is generallyhigher than for synthetics. Any one or all of these factors, or others,may well account for the difference in soil release results,particularly as to durability, between cellulosic/synthetic blendfabrics on the one hand and 100 percent synthetic fabrics on the other.

In view of the above, the principal object of the present invention isto provide 100 percent synthetic textiles which have improved grease orsoil release properties. Another object is to provide a novel processand composition for imparting highly advantageous grease releasecharacteristics to fabrics composed entirely of polyester and/or othersynthetic fibers which normally present grease release problems. Otherobjects will also be apparent from the following description of theinvention.

Broadly stated, the invention is based on the finding that soil releaseproperties of fabrics or other textile forms whose fiber content is madeup entirely of synthetic fibers can be improved, particularly as todurability to repeated laundering, by either of the following or acombination thereof:

1. scouring the textile in preparation for the application of the soilrelease finish using a special type of alkaline scour; and/or utilizingas the soil release finish a combination of polyacrylic acid and anotherpolymer, the latter being a water-insoluble swellable synthetic polymerwhich absorbs at least times its weight of water when immersed in anaqueous detergent solution for 2 minutes at 140 F. Preferably, the lastmentioned polymer is a copolymer of methacrylic acid and ethyl acrylatealthough other polymers can be used as discussed below. The best overallresults are obtained by using a combination of features (l) and (2) buteffective results are also obtainable when using only one of thesefeatures as described more fully below.

With respect to feature 2), it has surprisingly been found that thecombination of polyacrylic acid, in solution or emulsion forms. andother swellable synthetic polymers results in a synergistic effect withoutstanding soil release results. The effect is especially noticeableusing polyacrylic acid with methacrylic acid/ethyl acrylate copolymer inamounts such that the polyacrylic acid is about percent by weight of thecopolymer. However, other proportions may also be used, for example,l090% polyacrylic acid to 90-10% methacrylic acid/ethyl acrylatecopolymer. Other swellable polymers which meet the indicated waterabsorption test may also be used, in lieu of or in addition to themethacrylic acid/ethyl acrylate copolymer within the same generalproportions. The commonly assigned U.S. application, Ser. No. 604,649,filed Dec. 27, 1966, now abandoned; Ser. No. 681,092, filed Nov. 7,1967, now abandoned; Ser. No. 645,599, filed June 13, 1967, nowabandoned; and Ser. No. 683,139, filed Nov. 15, 1967, now US. Pat. No.3,521,993; describe soil release polymers which are suitable for presentpurposes and the subject matter of said applications is incorporatedherein by reference. These polymers may be defined as polymers whichabsorb at least about five times their weight of water under alkalineconditions or, more specifically, at least about 550 percent by weightof water when immersed in an aqueous detergent solution for 2 minutes at140 F. (pH about 8-12 Preferably, this polymer is an addition polymer ofat least one ethylenically unsaturated monomer having one or more acidgroups. Such'monomers include, for example, acrylic acid, methacrylicacid, itaconic acid, maleic acid, fumaric acid and the like. Monomerswhich contain groups which readily hydrolyze in water to form acidgroups also may be used, for example maleic anhydride. Preferably, theacid groups are all carboxylic acid groups. However, it is possible fora portion of them to be phosphoric acid (PC 11 or sulfonic acid (SO l-l)groups as well, by using monomers such as styrene sulfonic acid andphosphoric acid ester of glycidyl allyl ether. The polymers may bemanufactured by polymerizing the above monomers by any known means, forexample withfree radical or ionic catalysts. Alternatively, the polymersmay be made by polymerizing an ethylenically unsaturated monomer such asacrylonitrile or an acrylic ester and then hydrolyzing or otherwisemodifying the resulting polymer to convert the nitrile,

' ester or other groups to acid groups.

The polymers may contain relatively small amounts of monomers which donot include acid groups, for example olefins, e.g., ethylene andpropylene, aromatic olefins such as styrene and various methyl styrenes,acrylic and methacrylic esters such as methyl methacrylate and ethylacrylate, dienes such as butadiene and isoprene, vinyl halides, e.g.,vinyl chloride and vinylidene chloride, other acrylic monomers such asacrylamide and acrylonitrile, methyl vinyl ether; and the like. Ingeneral, the proportion of such non-acid monomers should not exceedabout 60 mole percent and preferably 40 percent. For maximum durability,it is preferred to use a system which leads to at least some degree ofcrosslinking so as to provide a matrix polymer with the other materialspresent.

Typical examples of water swellable polymers meeting the indicatedrequirements for present purposes include, in addition to polyacrylicacid and the copolymers of methacrylic acid and ethyl acrylate:copolymers of styrene and acrylic acid, copolymers of itaconic acid andacrylic acid; the copolymers of styrene, e.g., copolymers of styrene andmaleic anhydride; and methacrylic acid and acrylic acid terpolymers suchas terpolymers of methacrylic acid, butadiene and styrene; andterpolymers of monomethyl itaconate, acrylic acid and itaconic acid.

Preferably the waterabsorbing polymer is one which absorbs at leastabout 550 percent by weight of water. This is evidenced by verysubstantial swelling of the polymer although the polymer should not besoluble in alkaline solutions. The suitability of a polymer for useherein can be readily determined by measuring its water absorbingcapacity or swellability. To do this, fabric treated with the polymeronly is weighed, and the original weight of fabric is subtracted. Thefabric is then immersed in detergent solution for two minutes at 140 E,blotted dry with paper towels and then weighed. A correction is made forthe liquid absorption by the fabric itself by repeating the procedurewith uncoated fabric. The swelling is equal to: (weight gain incoating/dry weight of coating) X 100. A typical detergent solution whichmay be used for this purpose is 0.15% TIDE detergent in water. TIDEcomprises sodium lauryl sulfate 16%, alkyl alcohol sulfate 6%, sodiumpolyphosphate 30%, sodium pyrophosphate 17% and 31% sodium silicate andsodium sulfate combined.

The water absorbing (or swelling) characteristic of the soil releasepolymer is related to molecular weight. in general, low molecular weightpolymers of the type described above are water soluble whereas highermolecular weight polymers are insoluble in water but will swell. For themost part, suitable polymers, including both the polyacrylic acidcomponent and the other water-swellable polymer used therewith, willhave a number average molecular weight of 1,000 to 3,000,000, althoughthis is subject to some variation provided the desired degree of waterabsorption or swelling is realized without dissolution of the polymer.

Another factor affecting the water absorbing property or swellability ofthe polymer is the degree of cross-linking therein. The polymers usedherein are essentially linear polymers. As noted above, a certain degreeof cross-linking may be introduced into the polymers during subsequenttreatments. Although such cross-linking is not absolutely essential, itis desirable for durability. However, excessive cross-linking tends toconnect the polymer molecules into a rigid three dimensional networkwhich will not swell and this is not particularly useful for presentpurposes. Suitable cross-linking agents are formaldehyde, polyfunctionalalcohols, formaldehyde amine precondensates, polyfunctional epoxides,etc. These may be included as desired to improve durability.

The scour treatment of the inventions may be carried out in several waysusing alkaline scouring media to give a surface to which the greaserelease finish adheres more strongly and thus gives greater durabilityto laundering. It appears that the present scouring methods, asdistinguished from prior art scouring techniques, partially hydrolyzethe surface of polyester fibers so as to make more OH and COOH groupsavailable for reactivity. in any event, the alkaline pretreatments usedherein make the surface ofthe fabric more wettable and hydrophilic. Atest for the adequacy and effectiveness of the pretreatment is that thefabric, after scouring, must wet instantly with water, otherwise optimumsoil release properties are not realized. Equivalent results cannot beobtained by replacing the alkaline pretreatment with a wetting agentbefore or with the application of the soil release finish.

The alkaline scour of the 100 percent synthetic fabric, according to theinvention, is distinguishable from the conventional type of scouring towhich synthetic fabrics are normally subjected before the application offinishing agents. In the conventional treatment, the fabric is given adetergent scour with or without small amounts of a solvent like xyleneto remove surface dirt, oils, finishes, etc. The fabric, if a white isdesired, is then bleached, neutralized, and tinted with dyes and opticalbrighteners for better whitening. The treatment is insufficient,however, to obtain the results needed for adhesion of grease releasefinishes.

According to the invention, it has been found that the followingalkaline scours will give effective adhesion of the soil release finishand otherwise satisfactory results:

a. Caustic scour with the caustic dissolved in water and in the presenceof organic solvent such as xylene. Concentrations of the order of 2-15%NaOH, preferably 3-7%, and elevated temperatures up to the boil may beused (e.g., 200-2l2 F. for the aqueous scour). The time of treatment canbe varied but generally will run in the area of 15-45 minutes, typically30 minutes, the important requirement being that the fabric aftertreatment is characterized by instantaneous wetting with water. Thetreatment is usually accompanied by a fabric weight loss of from about0.5% to 7% indicative, to some extent, of hydrolysis.

b. Silicate scour using preferably 1 to 10% aqueous solutions of dryhigh alkalinity (pH 10 to 12) sodium silicates of the sesqui-,ortho-and/or meta-silicate types. This treatment is advantageouslycarried out at the boil for a period long enough to give a fabric thatinstantaneously wets with water, e.g., 30 minutes for treatment at theboil. This treatment gives even better results than the caustic scoureven though weight losses are usually lower and run from 0 to 2.5% byweight. Presumably the explanation does not depend on greater hydrolysiswith silicates because this would mean a greater weight loss. Thepresence of silica sio, which is a powerful absorbent, might be part ofthe explanation, it being noted that the acid neutralized product of NaSiO is H SiO which may dehydrate to $0,.

It will be appreciated that, in the case of fabric scoured by caustic orsilicate as noted above, the invention contemplates the possibility ofusing polyacrylic acid and/or any one or more of the soil releasepolymers referred to earlier as the primary soil release finish, thescour pretreatment resulting in a percent synthetic fabric whichdemonstrates much more durable and otherwise better soil releaseproperties.

In lieu of the scouring pretreatment but preferably in combinationtherewith for optimum results, the invention also contemplates using amixture of polyacrylic acid and one or more of the other soil releasepolymers mentioned above for soil release purposes to produce asynergistic effect. As noted, the combination of caustic or alkalinesilicate scour and polyacrylic acid/polymer finish gives the bestresults and is preferred from the standpoint of finish durability tolaundering and soil release properties. However, just the use of thecombination of polyacrylic acid and other polymer, preferablymethacrylic acid/ethyl acrylate copolymer, on conventionally scoured 100percent synthetic fabric gives highly improved soil release and may beadequate in many instances.

Additives may be included with the soil release finish to improve hand,grease release and durability. The use of plasticizers in the soilrelease finish employed herein represents a particularly importantaspect of the invention in order to obtain optimum results as to greaserelease, hand and other important properties.

For present purposes, the term plasticizer" is intended to mean anymaterial which, when used as described herein, increases flexibility,workability or distensibility of the coating polymer. Plasticizerssuitable for use are described in the copending application Ser. No.733,332, filed May 31, 1968, now abandoned, by Maggiolo et al. and thesubject matter of said application is incorporated herein by reference.Typically useful plasticizers are butyl hexyl phthalate, diisooctyloleate, tri-Z-ethylhexyl trimellitate, diisodecyl phthalate, triisodecyltrimellitate, trioctyldecyl trimellitate, triisooctyl trimellitate,diisodecyl adipate, tricresyl phosphate, diisooctyl sebacate, dicaprylphthalate, N-octyl-N-decyl adipate, di-2ethylhexyl azelate, triphenylphosphate, butyl and butyl glycollic phthalate, methyl and ethylglycollic phthalate, dihexyl azelate, tetrahydrofurfuryl oleate,diethylene glycol dipelargonate, dibutyl sebacate, butyl benzylphthalate, dibutyl phthalate, di- 2-ethylhexyl phthalate, epoxytallate-Plastolein 9214, diisooctyl azelate, diisooctyl adipate,diisooctyl phthalate, tri (N-octyl/decyl) trimellitate, Plastolein 9066LT, Plastolein 9750 polymeric (2200MW), Plastolein 9765 polymeric(3500MW), modified phthalate Santicizer 213, Santicizer 481, modifiedphthalate Santicizer 214, Plastolein 9078 LT, Plastolein 9232 epoxy,Santocet No. 1 reactive plasticizer, Plastolein 9722 polymeric (IOOOMW),Plastolein 9717 polymeric (850MW), Plastolein 9730 polymeric (1100MW),

9-cyclohexyl stearic acid, 9-phenyl stearyl nitrile, 9-phenyl stearylamine (primary), N,N-Dimethyl-9-stearyl amide, N-(2Hydroxyethyl)-9-phenyl stearyl amide, 9-(4-hydroxy-phenyl) stearic acid,phthalic acid half ester of l-hexadecyloxy-2- hydroxy dodecane,isophthalic acid half ester of l-hexadecyloxy-2-hydroxy dodecane,n-hexadecyl-9-phenylstearate, 9-(4-biphenyl) stearic acid,9-(4-phenoxyphenyl) stearic acid, 9-(4-benzylphenyl) stearic acid, andphenyl stearic acid.

Other additives which may be used herein include materials such ascaprolactam blocked urethane prepolymer emulsions of nonionic naturecontaining a curing polyol (Nopco D602 and D607) are useful to improvedurability to laundering. High molecular weight urethane emulsions ofnonionic nature such as the Wyandotte products E-207A and E-503,are'also useful in this regard. Acrylic terpolymers of low pH (e.g.,2-4) such as the material known as R-992 90 B (National Starch) and thepolymers 2507 High Styrene Type and 2600 X140 Acrylic Type (both B. F.Goodrich) are useful additives to the soil release finish. This is alsotrue for D-623 (Nopco) which is a one-component blocked urethaneprepolymer emulsion which includes no curing polyol; acrylic andstyrene/butadiene type polymers in anionic emulsion. Typically thesevarious additives, for example, caprolactam blocked urethane prepolymersare used in concentrations (solids) of the order of 0.2 to 1.0%, andgenerally within the more limited range 0.4% to 0.7%. The Nopcourethanes may be prepared under US. Pat. No. 3,245,961.

The fabric may also be treated with primers before application of thesoil release finish. Typical primers include those listed above underadditives as well as epoxy silanes (e.g., Union Carbide's A] 87,glycidoxy propyl trimethoxy silane). When used, the primers aregenerally applied in the form of aqueous solutions or dispersions inconcentrations of 0.1 to 0.5%, preferably 0.2%, by weight. Solid pickupamounts to about 0.05 to 0.3% based on the dry fabric weight beforetreatment.

in a further embodiment of the invention, ammonia vapor has also beenused to advantage in producing a fabric of good soil release properties.This is accomplished by padding the fabric with dispersion of the soilrelease polymer or mixture thereof, exposing the fabric while wet tosteam and ammonia vapors and then drying and curing.

In a preferred embodiment, the invention involves impregnating the 100percent synthetic fabric, advantageously but not necessarily after analkaline scour as aforesaid, with an aqueous solution or dispersion ofpolyacrylic acid and a 60/40 copolymer of methacrylic acid and ethylacrylate (referred to elsewhere herein for convenience as MAA/EA), aplasticizer and an additive as described above. The monomer proportionsin the copolymer may be higher or lower than indicated (e.g., from -90%methacrylic acid) but the 60/40 copolymer seems to offer optimum resultsin the usual case. A particularly preferred composition for impregnatingthe fabric (by padding, spraying or otherwise), comprises, on a weightbasis, from l3% of the MAA/EA copolymer (60/40), 0.5% to 1.5% solids of100% polyacrylic acid (e.g., K-702, B. F. Goodrich) and from 1.0% to 3%solids of an aqueous plasticizer emulsion of triisodecyl trimellitate(e.g., Moreflex 530, Pfizer), and 0.4 to 0.7% solids of Nopco D-602additive. Usually the amount of polyacrylic acid solids is about 50% ofthe MAA/EA copolymer whilethe amount of plasticizer solids is normallyabout the same as the amount of MAA/EA. These ratios are also generallyapplicable when other polymers are used in lieu of the MAA/EA althoughadjustments may be necessary to obtain optimum results with anyparticular set of components.

The fabric may be in the wet or dry state when padded with the soilrelease composition. However, if processed in the wet state, the solidspickup should be at least twice that for dry cloth. The treatment of wetfabric has the advantage of saving the step of drying the fabric beforeapplication but care must be taken to evenly squeeze out excess moisturefrom the fabric to insure uniform pickup when the fabric is treated inthe wet state.

The amount of the composition applied to the fabric can be widely variedand is dependent on such factors as the nature and construction of thefabric, its intended use, etc. Usually, however, wet pickup will fall inthe range of 30-100% by weight of the fabric if the latter is initiallyin the dry state while pickup should be higher if the fabric is treatedwet as aforesaid. After impregnation, this fabric is dried, usually at190-300 F for l5 minutes, and cured at 300380 F. for a few seconds to 15minutes. The drying procedure provides a degree of partial cure, usuallyabout 25 percent, and forms at least some cross-linking in the soilrelease finish.

The invention may be used to improve the soil release properties of anytype of percent synthetic fabric, e.g., knitted, woven, nonwoven orcombinations thereof. It is of particular advantage in the case offabrics made up entirely of polyester fibers although 100 percent nylonand acrylic fabrics or fabrics composed of blends of polyester, nylon,acrylic and/or other hydrophobic synthetic fibers may also beeffectively processed according to the invention.

The invention is illustrated by the following examples wherein partsand/or percentages are on a weight basis in a water solution ordispersion. Soil release properties were determined in these examples bysoiling the fabric specimens with black oil, mineral oil, clean motoroil and French dressing. After soiling, the specimens were washed in ahome laundry agitator type top loading automatic washing machine set atF. on the wash/wear cycle using a low sudsing detergent (e.g., ADD, pHabout 10). After washing in a 35 minute total cycle on the wash-wearcycle, the specimens were tumble dried at -170 F. After conditioning,the specimens were placed on a black surface under a fluorescent light.The specimens were visually, rated against a series of photographicstandards with numerical ratings as follows:

Class 5 No staining Class 4 -Slight, but not appreciable staining Class3 -Noticeable staining Class 2 Very noticeable staining Class 1 -Veryextreme staining In the examples given, where data is shown for 10 or 20launderings, the fabric specimen was laundered nine or 19 times,respectively, stained and washed one time before rating. These extensiveprelaunderings" were used to determine durability of the soil releasefinish to repeated washing. In all examples, unless otherwise indicated,conventionally scoured fabrics were employed. The conventional orregular scouring procedure usually consists of scouring cloth at 203 F.for about V2 to 1 hour in an emulsifier or detergent to remove any oilsor dirt. A typical procedure involves: 0.13% Hipochem MS (a phosphateester made by High Point Chemical Co.) emulsifier and 0.02% HypochemHipochem ST (tetrasodium salt of ethylene diamine tetraacetic acid madeby High Point Chemical Co.)- sequestrant.

EXAMPLE 1 A. A 100% Dacron tricot was padded with an aqueous dispersion(8% solids) of methacrylic acid/ethyl acrylate copolymer (60/40), driedfor 2 minutes at 200 F. and then cured at 350 F. for 2 minutes.

B. The procedure of paragraph (A) was repeated on a similar 100 percentDacron tricot using an aqueous solution (8 percent solids) ofpolyacrylic acid.

C. The procedure of paragraph (A) was repeated using an aqueousdispersion of polyacrylic acid (5 percent solids) and 3 percent solidsmethacrylic acid/ethyl acrylate copolymer.

The thus treated fabric specimens (approximately 75 percent wet pickupin each case) were then soiled and tested for soil removal. Thefollowing results were obtained (after 10 launderings):

Clean French Treatment Black Mineral Motor Dressing Oil Oil Oil A 2.5 55 5 B 3.0 4 3 4 C 4.0 5 5 5 This shows the synergistic effect obtainedwith the combination of polyacrylic acid and MAA/EA copolymer indurability of finish and soil release, it being noted that only 3%MAA/EA is used with percent polyacrylic acid in Treatment A and theresults of this treatment are as good as, or better than, Treatment Awhere 8% MAA/EA is used and much better than Treatment B where 8 percentpolyacrylic acid is used.

EXAMPLE 2 A. 100% Dacron tricot was padded with an aqueous l percent(solids) dispersion of the methacrylic acid/ethyl acrylate copolymerused in Example 1 and left wet (i.e., the drying and curing of Example 1were omitted;

B. Paragraph (A) of this example was repeated except that a 1 percentsolution of polyacrylic acid was used in lieu of the copolymer, thefabric being left wet;

C. Paragraph (A) of this example was repeated except that the padcomprised 1 percent (solids) of the copolymer and 1 percent solidspolyacrylic acid, the fabric being left wet.

The wet fabric specimens were all exposed to vapors of steam and ammonia(600 cc. NH,OH in gals. water) at approximately 190 F. for 5 minutes,dried 2 minutes at 200 F. and cured 2 minutes at 350 F.

On testing for stain removal of black oil as in Example 1, the followingresults were obtained after 10 launderings:

Treatment Rating A 3 B l These results show the improvement obtainingfrom the combination of l) MAA/EA copolymer and polyacrylic acid for thefinish and (2) ammonia vapor treatment.

EXAMPLE 3 Example 1 was repeated using bar on bar tricot fabric composedof 57% T-57 Dacron and 43 percent nylon and the following padcomposition:

A. 1% solids MAA/EA copolymer in water B. 1% solids AA in water C. 1%solids AA plus 1% solids MAA/EA copolymer in water.

As will be recognized, the abbreviations MAA/EA and AA have been usedabove and are employed elsewhere herein, for convenience, to designate,respectively, the 60/40 methacrylic acid/ethyl acrylate copolymer andpolyacrylic acid.

The results ofstain removal after 10 launderings were as follows:

Cleun French Treatment Black Mineral Motor Dressing Oil Oil Oil A 2.54.5 3.0 4.5 B 1.0 2.5 2.5 2.5 41 5.0 5.0 5.0

Untreated 1.0 2.5 1.0 1.0

Here again, the improvement resulting from the combined use of MAA/EAand AA are to be noted. it should also be noted that the ratings of theuntreated fabrics used in this example apply to the other examples whichuse the same fabric and the same scour.

EXAMPLE 4 A. A bar on bar tricot composed of 57% T-57 Dacron/43% nylonwas padded with 0.5% solids AA, 0.5% solids MAA/EA, and 2.0% solidsemulsified TIDTM in water and left wet.

B. Paragraph (A) of this example was repeated on another similar fabricusing a pad of 0.5% solids AA, 1.0% solids MAA/EA, and 2.0% solidsemulsified TIDTM in water.

C. Paragraph (A) of this example was repeated using a pad of 1.0% solidsMAA/EA, plus 2.0% solids emulsified TIDTM in water.

The TIDTM" referred to above was an emulsion of Morflex 530 (triisodecyltrimellitate).

All of the fabric specimens were exposed while wet to vapors of steamand ammonia (600 cc. Nl-LOH per 20 gals. water) at approximately 190 F.for 2 minutes, dried 2 minutes at 200 F. and cured 2 minutes at 350 F.

The results of stain removal (10 launderings) are given below:

Treatment Black Oil Clean Motor Oil A 2.5 3.0 B 4.0 5.0 C 3.0 5.0

In the above example, the TIDTM functioned to improve hand while it willbe noted that better soil release was attained with Treatment (B) usingthe higher total solids of MAA/EA plus AA vs. Treatment (A). The ratioof 50% AA on the weight of the MAA/EA to produce a synergistic effect isalso noted in Treatment (B).

EXAMPLE 5 A. Dacron tricot was padded with the following composition:

1% solids MAA/EA, 0.5% solids AA and 1% solids emulsified TIDTM B. Asimilar fabric was padded with the following composition:

1% solids MAA/EA, 0.5% solids AA and 1% solids phenyl stearic acid Bothfabrics were scoured before application of soil release with 3% NaOHsolution at F., 15 minutes (2.5% weight loss) rinsed, neutralized in 1%acetic acid, rinsed, dried 2 minutes at 200 F.

Both fabrics, after padding with the indicated soil releasecompositions, were dried 2 minutes at 200 F. and cured 45 seconds at 380F.

Results of stain removal l0 launderings) were as follows:

Clean French Treatment Black Mineral Motor Dressing Oil Oil Oil A 4 5 55 B 3 4.5 5 4.5

The TITDM and phenyl stearic acid used in this example gave the fabric asofter hand. In both instances the soil release was good, it being notedthat black oil is an extremely severe test soil.

EXAMPLE 6 Fabric: 57% T-57 Dacron/43% Nylon bar on bar tricot.Procedures: A. Caustic scoured as in Example 5, then padded with 1%solids MAA/EA, 0.5% solids AA and 1% solids emulsified TIDTM in water.B. Same as A except no caustic scour. Results of stain removal, 10launderings.

Clean French Treatment Black Mineral Motor Dressing Oil Oil Oil A 4.04.0 5.0 4.0 B 3 .0 4.0 3.0 4.0

This example shows the advantage of caustic scour before treatment withthe soil release finish.

EXAMPLE 7 Fabric: 57% T-57 Dacron/43% Nylon bar on bar tricotProcedures:

A. Scour for 30 minutes at 203 F. in 10 percent solids solution in waterof anhydrous sodium metasilicate, rinsed, neutralized in 2 percentacetic acid at room temperature, rinsed and dried 2 minutes at 200 F.

B. Regular scour.

The fabrics obtained by scouring procedures A and B were All fabrics,after scouring as indicated, were padded with 3% both padded with 1percent solids MAA/EA plus 0.5 percent solids MAA/EA, 1.5% solids AA,and 3.0% solids emulsified solids AA and 1 percent solids emulsifiedTIDTM, dried 2 TIDTM, dried 2 minutes at 250 F. and cured 45 seconds atminutes at 250 F. and cured 45 seconds at 380 F. 380 F.

Results of stain removal after 1, l and 15 launderings were 5 asfollows:

These results point up the advantage of an alkaline silicate The resultsof stain removal after and launderings: scour over the conventionalscour. 1-5

' Clean French EXAMPLE 8 Treat Black Mineral Motor Dressing ment Oil OilOil Fabric: 57% T-57 Dacron/43% Nylon bar on bar trlcot. 10 1o 10 10 1010 o 10 Procedures: 20 A 3.0 2.5 3.0 2.5 3.0 2.5 3.0 2.5 s 4.0 4.5 4.04.0 5.0 5.0 4.0 4.0 A. Pad 3.0% sollds MAA/EA, 1.5% solids AA and 3.0% C40 10 to 4.0 M M 10 1o solids emulsified TIDTM in water.

Pad Same as A except add 064% solids Nopco D'6O7 These results show thesuperiority of the alkaline scours B i and C over regular scouring ingiving better and more durable C. Prime fabric with 0.64% sollds aqueousdlsperslon of 5 grease release over extended launderings Nopco D-607,dry 2-l/2 minutes at 250 F. Then apply A finish. EXAMPLE 11 In eachinstance, the fabric after application of A, B or C, was F b dried 2%minutes at 250 F. and cured 45 seconds at 380 F. T 51 d bl D l Theresults of stain removal after 1, l0 and 20 launderings are .1 P g {Sacronlpo yester shown below: E L MU EEL Black Oil Mineral 011 CleanMotor 011 French Dressing Treatment:

It is to be noted that the urethane additive, whether added C. l00%disperse dyeable Fortrel polyester with the grease release finish or asa primer therefor, improved Procedure: All fabrics were padded with 3.0%solids the durability of the soil release properties on extended laun-MAA/EA, plus 1.5% solids AA, plus 3.0% solids emulsified derin gs. TIDTMin water, dried 2 minutes at 250 F. and cured seconds at 380 F. EXAMPLE9 The results of stain removal after ten launderings were: Fabric: 57%T-5 7 Dacron/43% Nylon bar on bar tricot 45 Procedures: Clea A. Pad on3.0% solids MAA/EA, plus 1.5% solids AA plus 5:? .1 '55' 3.0% solidsemulsified TIDTM in water. A 2.5 2.5 2.5 2.5 B. Pad on 0.2% aqueoussolution of epoxy silane A-l87 (U- B nion Carbide), dry 2% minutes at250 F. Then apply A C finish. In each instance, the fabric afterProcedure A or B, was dried i example shows h there ls some vanauon "Eeffect 2% minutes at 250 F., and cured for 45 seconds at 380 F. pendmgon the synthetlc fibers employed In pamcular the basic dyeable Dacronfibers seem to give a better effect than The results of stem removalafter one and 10 launderlngs the disperse dyeable polyester fibers. Thisy be due to were:

Clean Hench greater wettability in the basic dyeable fibers or a higherener- Black Mineral Dressing gy surface which is more compatible to thesoil release finish. ment Oil Oil Oil V V 1 l0 1 l0 1 1o 1 10 A 4.5 4.05.0 3.0 5.0 4.5 5.0 4.0 s 4.0 4.0 5.0 5.0 5.0 5.0 5.0 5.0

These results show that use of a silane primer is beneficial to M" L theresults obtained.

EXAMPLE 10 Fabric: 57% Dacron/43% Nylon bar on bar tricot. Procedure:Fabric: 57% T-57 Dacron/43% Nylon bar on bar tricot. A. Pad 3.0% solidsMAA/EA, 1.5% solids AA, and 3% Procedures: solids emulsified TIDTM. A.Regular scour as in Example 7. B. Same as A except include add 0.42%solids Nopco B. Scoured in 10% anhydrous sodium metasilicate aqueousD-602 urethane in pad composition. All fabrics before solution 30minutes at 203 F., rinsed, neutralized in 2% soil release applicationwere scoured 30 minutes at 203 acetic acid, rinsed and dried 2% minutesat 250 F. (1.2% F. in a 10% anhydrous sodium metasilicate solution,weight loss). rinsed, neutralized in 2% acetic acid, rinsed and dried 3C. Scoured in 5% caustic (NaOl-l) solution for 30 minutes at minutes at250 F. (1.9% weight loss).

203 F., rinsed, neutralized in 2% acetic acid, rinsed, and The soilrelease finish was dried 2 minutes at 250 F. and dried minl ss at 9 Fsureqfi seconds 512%? E The results of stain removal after 10 and 20launderings were:

Clean French Trent Black Mineral Motor Dressing ment Oil Oil Oil 10 20 I20 I0 20 A 4.0 3.0 3.0 4.0 3.0 4.0 3.0 4.0 B 4.0 4.0 4.5 4.5 5.0 4.5 5.04.5

The above results show that the urethane additive improves thedurability of the finish to laundering.

EXAMPLE 13 Fabric: 57% Dacron/43% Nylon bar on bar tricot.

Procedures:

A. Scour in 3% aqueous anhydrous sodium orthosilicate to 0.75% weightloss.

B. Scour in 6.0% aqueous anhydrous sodium metasilicate to 1.5% weightloss.

C. Scour in 10% aqueous liquid sodium silicate to 0.25%

weight loss.

D. Scour in 15% aqueous liquid potassium silicate, no measurable weightloss. All scouring treatments were for minutes at 203 F. after which thefabrics were rinsed, neutralized in 2% acetic acid, rinsed and dried 2%minutes at 250 F.

All fabrics were then padded with 2.0% solids MAA/EA, 1.0% solids AA,and 2.0% solids emulsified TIDTM, dried 2 minutes at 250 F. and cured 45seconds at 380 F.

The results of stain removal after 10 and 20 launderings were:

Clean French Treat Black Mineral Motor Dressing ment Oil Oil Oil 10 2010 20 10 20 I0 20 A 4.0 4.0 5.0 4.5 5.0 5.0 5.0 5.0 B 4.0 4.0 5.0 4.55.0 5.0 5.0 5.0 C 3.0 3.0 5.0 4.5 5.0 4.5 5.0 4.5 D 3.0 3.0 5.0 4.5 5.04.5 5.0 4.5

The above results show the superiority in performance of productsinvolving procedures (A) and (B) using the more alkaline treatments withslight weight losses.

EXAMPLE 14 Fabric: 57% T-62 Dacron/43% Nylon bar on bar tricot.

Procedures:

A. Aqueous pad composition containing 2% solids MAA/EA plus 1% solidsAA, plus 2% solids emulsified TIDTM.

B. Same pad as A except include in the pad add 0.42% solids E-207A fromWyandotte Co.) a completely reacted high molecular weight urethanepolymer in nonionic emulsion.

C. Same pad as A except include add 0.4% solids E-503 from (WyandotteCo.), a completely reacted high molecular weight urethane polymer innonionic emulsion.

All fabrics were padded, dried 2 /2 minutes at 250 F. and cured 45seconds at 380 F.

The results of stain removal after 10 and 20 launderings were:

Clean French Trent Black Mineral Motor Dressing ment Oil Oil Oil A 2.52.5 4.0 3.0 4.0 3.0 4.0 3.0 B 2.5 3.0 4.5 5.0 4.0 4.5 4.5 4.5 C 2.5 3.04.0 4.0 4.0 4.0 4.0 4.5

These results again show the improved durability of the finish toextended launderings when a urethane polymer is used as an additive.

EXAMPLE 15 Fabric: Nylon tricot. t s qurs; A. Aqueous pad compositioncontaining 1% solids MAA/EA plus 1% solids emulsified TIDTM. B. Aqueouspad containing 1% solids AA plus 1% solids emulsified TIDTM. C. Aqueouspad containing 1% solids MAA/EA, plus 0.5%

solids AA, and 1.0% solids emulsified TIDTM. All fabrics were padded,dried 2 minutes at 250 F. and cured 45 seconds at 380 F.

The results of stain removal after one and 10 launderings were:

Treatment Black Oil A 1.0 1.0 B 3.0 3.0 C 4.0 5.0

These results show the synergistic effect of using the combination ofMAA/EA and AA on Nylon. After 20 launderings, fabric C had a 5 rating.

EXAMPLE 16 Fabric: 57% T-57 Dacron/43% Nylon bar on bar tricotProcedures:

A. Regular scoured fabric, 38 lbs., left wet for soil release finish.

B. Silicate scour, 38 lbs. cloth scoured in a 6% solution of anhydroussodium metasilicate in 360 gals. water volume at 203 F., 30 minutes in acommercial dye beck, rinsed with water, neutralized in 0.6% acetic acid,rinsed in water, squeezed and left wet for soil release finish (1%weight loss).

All fabrics were padded in wet state with aqueous dispersion containing2.0% solids MAA/EA, 1% solids AA, 2.0% solids emulsified TIDTM, and0.42% Nopco D-602 urethane. All were dried in a commercial pin tenterframe at 23 yards/min. speed at 225 to 300 F. in a graduated temperatureoven, and then passed at the same speed into a gas heated over for 15seconds at 380 F. (cloth temperature).

All fabrics were stained with nine oily stains, and given 1, 10

and 20 launderings.

7 The results of stain removal were:

ONE LAUNDERING 3-1 Bacon Fr. Motor Mineral Mayon- Corn Black 011 FatDress. O11 O11 Butter nalse 011 Oil Treatment 5 5 5 4. 5 5 5 5 5 2. 5 B5 5 5 5 5 5 5 5 4 Reg. scoured, no soil releas 1 1 1 1 1 1 1 1 1Silicate scoured, no sol1re1ease.. 4. 5 3 3 3 3 3 3 3 3 TEN LAUNDERIN G82 2 2 4 i 3 2 2 2 4. 5 4. 5 5 4. 5 4. 5 4. 5 4. 5 4. 5 Reg. scoured, nosoil raises 1 1 1 1 1 1 1 1 Slllcate scoured, no soil release" 4. 5 2 33 3 3 3 2 3 TWENTY LAUNDERIN GS A 3 2. 5 2. 5 3 3 3 3 2. 5 1 B 5 4 5 5 55 5 5 3 Reg. scoured, no soil release... 1 1 1 1 3 1 1 1 1 Silicatescoured. no soil release 4 3 3 3 4 3 3 3 5 13 These results demonstratetheoutstanding durability of the silicate treated fabric and thesignificant advantages of this scouring treatment over the regular scourfor grease release.

EXAMPLE 17 Fabric: 57% T-62 Dacron/43% Nylon bar on bar tricotProcedures:

A. 55 yards scoured in a standard commercial dye beck in 360 gals. waterwith regular scour.

B. 50 yards scoured in beck containing 360 gals. water containing:Xylene emulsifier 0.143% Hipochem MS (High Point Chemical Co.)Sequestrant 0.018% Hipochem ST (High Point Chemical Co.) Emulsifier0.143% Caustic 0.143% Xylene 0.72% Boil 1 hour C. 50 yards regularscoured fabric were scoured in 360 gals. water containing 1.5% anhydroussodium metasilicate and processed the same as in Example 16 for thesilicate process.

All fabrics were bleached with acid chlorine type bleach before theabove scours. All fabrics were tinted together with blue dye and opticalbrightener, after the above scours, and left in the wet state.

All fabrics were then padded wet (after squeezing with padder rolls)with an aqueous pad composition containing 2.2% solids MAA/EA, 1.1%solids AA, 2.2% solids emulsified TlDTM, and 0.46% solids Nopco D-602urethane. They were then dried in a commercial pin tenter frame at 25yards/min. under the same conditions as in Example 16.

All fabrics were stained with the same stains as in Example 16 andwashed the same. The results on the scours B and C were similar to ScourB in example 16, and showed the superior performance of the two alkalinescours opposite the regular Scour A. On Scour B, the followingadditional stains were applied and completely removed in laundering at 1F.:

urine anti-perspirants egg yolk grape juice ketchup coffee blood (driedon cloth overnight) It will be appreciated that various modificationsmay be made in the invention describedhere in l leng th e scope of 14the invention is defined in the following claims herein.

We claim:

1. A process for improving the soil release properties of a 100 percentsynthetic textile which comprises impregnating the same with a mixtureconsisting essentially of 10 to 90 percent of polyacrylic acid and 90 to10 percent of an essentially linear water-insoluble swellable syntheticpolymer of an ethylenically unsaturated monomer having at least one acidgroup which polymer absorbs at least 550 percent of water when immersedin an aqueous solution for 2 minutes at 140 F. then drying and curing.

2. The process of claim 1 wherein the polymer is a copolymer ofmethacrylic acid and ethyl acrylate.

3. The process of claim 2 wherein said textile is a fabric comprisingpolyester fibers.

4. The process of claim 1 wherein said mixture is applied to saidtextile as an aqueous composition.

5. The process of claim 1 wherein the textile, after impregnating butbefore drying, is exposed to treatment with steam and ammonia vapor.

6. The process of claim 1 wherein said mixture includes a plasticizer.

7. The process of claim 1 wherein said mixture includes a furtheradditive for improving hand, soil release and durability.

8. The process of claim 1 wherein the synthetic textile comprises basicdyeable polyester fibers.

9. The process of claim 1 wherein the synthetic textile comprisessynthetic fibers which have been modified to have in- -creased surfaceenergy.

10. The product obtained by the process of claim 1. 11. A process forimparting soil release properties to a 100 percent synthetic textilewhich comprises subjecting said textile to an alkaline scour until saidtextile is immediately wettable and then applying a soil release finishthereto consisting essentially of 10 to 90 percent of polyacrylic acidand 90 to 10 tion for 2 minutes at F. then drying and curing.

12. The process of claim 1 1 wherein the scour is selected from thegroup consisting of caustic and silicate.

13. The product obtained by the process of claim 1 1.

2. The process of claim 1 wherein the polymer is a copolymer ofmethacrylic acid and ethyl acrylate.
 3. The process of claim 2 whereinsaid textile is a fabric comprising polyester fibers.
 4. The process ofclaim 1 wherein said mixture is applied to said textile as an aqueouscomposition.
 5. The process of claim 1 wherein the textile, afterimpregnating but before drying, is exposed to treatment with steam andammonia vapor.
 6. The process of claim 1 wherein said mixture includes aplasticizer.
 7. The process of claim 1 wherein said mixture includes afurther additive for improving hand, soil release and durability.
 8. Theprocess of claim 1 wherein the synthetic textile comprises basic dyeablepolyester fibers.
 9. The process of claim 1 wherein the synthetictextile comprises synthetic fibers which have been Modified to haveincreased surface energy.
 10. The product obtained by the process ofclaim
 1. 11. A process for imparting soil release properties to a 100percent synthetic textile which comprises subjecting said textile to analkaline scour until said textile is immediately wettable and thenapplying a soil release finish thereto consisting essentially of 10 to90 percent of polyacrylic acid and 90 to 10 percent of an essentiallylinear water-insoluble, swellable synthetic polymer which absorbs atleast 550 percent of its weight of water when immersed in an aqueousdetergent solution for 2 minutes at 140* F. then drying and curing. 12.The process of claim 11 wherein the scour is selected from the groupconsisting of caustic and silicate.
 13. The product obtained by theprocess of claim 11.